CN113897095A - Thermochromic ink and preparation method thereof - Google Patents
Thermochromic ink and preparation method thereof Download PDFInfo
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- CN113897095A CN113897095A CN202010633594.5A CN202010633594A CN113897095A CN 113897095 A CN113897095 A CN 113897095A CN 202010633594 A CN202010633594 A CN 202010633594A CN 113897095 A CN113897095 A CN 113897095A
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- 239000000843 powder Substances 0.000 claims abstract description 139
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- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 5
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses thermochromic ink which comprises the following components in parts by weight: 12-18 parts of a connecting material, 2.5-4.5 parts of a cross-linking agent, 45-78 parts of a solvent, 2.5-4 parts of a flatting agent, 1.0-3.5 parts of a wetting agent, 1-10 parts of a temperature-sensitive color-changing powder mixed glue, 8.5-12 parts of an antifoaming agent, 0-8 parts of a curing agent, 15-25 parts of a diluent, 1-3 parts of an antioxidant, 1-2.5 parts of a nano-grade filler, 1-3 parts of a dispersing agent and 1-10 parts of a temperature-sensitive color-changing powder. The thermochromic ink prepared by the invention has the advantages of higher accuracy and sensitivity, high air drying speed, high adhesive force, excellent high-temperature and low-temperature resistance, sensitive color change, no problems of migration, falling or reverse sticking and the like when being used for sticking character anti-counterfeiting marks on outer packing boxes, and good water resistance.
Description
Technical Field
The invention belongs to the technical field of printing ink, and particularly relates to thermochromic printing ink and a preparation method thereof.
Background
At present, conventional non-color-changeable ink is adopted to print in the leather industries such as PVC, TPU, PU synthetic leather, microfiber, double-layer leather and the like, and trademarks, brands and pictures and texts of the industries such as toys, daily necessities, packages, electronic products and the like, and the conventional ink does not change color, has no specificity and thus does not have the functions of anti-counterfeiting and warning. The early thermochromic ink mostly uses inorganic thermochromic materials, and the principle of the inorganic thermochromic material is that reversible color changes are generated by pigment crystal form transformation and ligand geometric configuration changes, such as: CoCl2*2C6H12N4*10H2The reversible change of the crystal between pink or sky blue is generated by the dehydration of O at the temperature of 39.6 ℃, and the thermo-sensitive color change mechanism of the crystal utilizes the inherent property of the substance; however, the color and temperature of the desired change cannot be selected independently, and the color change is usually more dispersive, has less color difference and great toxicity, and thus has larger limitation.
With the rapid development of the packaging industry in recent years in China, the ink industry in China is greatly expanded. Particularly, in recent years, the Chinese packaging industry pursues exquisite printing, and meanwhile, the thermochromic ink has no harm to human health, has little pollution to the environment and is more environment-friendly and can be widely applied to packaging anti-counterfeiting materials such as printed food, medicines, cigarette and wine anti-counterfeiting marks and the like. The thermochromic ink is a special ink which can change the color of a pigment along with the change of temperature, and can be particularly divided into reversible ink and irreversible ink, wherein the irreversible ink in the market mainly takes inorganic substances as the color-changing pigment, most of the inks contain heavy metals, and the color-changing temperature is high. The thermochromic ink can be applied to screen printing, the product design demands that the color changes between a high-temperature environment and a low-temperature environment, and the thermochromic ink is mostly applied to series products of human body temperature sensing and can also be used as an anti-counterfeiting design. The thermochromic ink is slightly irritant to the respiratory tract for skin, should be sealed during transportation, and should maintain good ventilation condition in the printing operation environment. After the printing ink is completely dried, no peculiar smell or irritation exists, and the packaging specification standard of safe toys and food is met.
However, the color of the current thermochromic ink is insensitive and has long color restoration time, rapid color change cannot be realized, the anti-counterfeiting effect is influenced, and when the thermochromic material is applied to the ink, the problems of low adhesive force and the like, difficult wetting and slow drying of the ink and the like often exist.
Disclosure of Invention
The invention aims to provide thermochromic ink and a preparation method thereof, wherein the thermochromic ink has the advantages of capability of realizing rapid color change, good ink adhesion, rapid drying and easy wetting.
In order to achieve the above object, according to one aspect of the present invention, there is provided a thermochromic ink comprising the following components in parts by weight: 12-18 parts of a connecting material, 2.5-4.5 parts of a cross-linking agent, 45-78 parts of a solvent, 2.5-4 parts of a flatting agent, 1.0-3.5 parts of a wetting agent, 1-3 parts of an antioxidant, 8.5-12 parts of an antifoaming agent, 0-8 parts of a curing agent, 15-25 parts of a diluent, 1-10 parts of a temperature-sensitive color-changing powder, 1-2.5 parts of a nano-grade filler, 1-3 parts of a dispersing agent and 1-10 parts of a temperature-sensitive color-changing powder mixed glue.
According to the invention, the thermochromic ink comprises the following components in parts by weight: 14-16 parts of a binder 3-4 parts of a cross-linking agent, 50-70 parts of a solvent, 2.8-3.5 parts of a flatting agent, 1.5-3 parts of a wetting agent, 1.5-2 parts of an antioxidant, 10-11 parts of a defoaming agent, 2-3 parts of a curing agent, 18-22 parts of a diluent, 4-8 parts of a temperature-sensitive color-changing powder, 1.5-2.0 parts of a nano-grade filler, 1.5-2 parts of a dispersing agent and 4-8 parts of a temperature-sensitive color-changing powder mixed glue.
According to the present invention, the binder is a transparent thermosetting resin including one or more of epoxy resin, acrylic resin, and urethane resin. Preferably, the viscosity of the binder is 8-10Pa.S/30 ℃. Preferably, the curing agent is one or more of imidazoles, acid anhydrides, polyester resins, liquid polyurethanes, and polyisocyanates. The curing agent and the binder are matched to form a two-component system, and when the binder is epoxy resin, the curing agent is imidazole, acid anhydride, polyester resin or liquid polyurethane curing agent; when the connecting material is polyurethane resin and/or hydroxyl acrylic resin, the curing agent component is polyisocyanate; when the main body of the binder is epoxy acrylic resin, the curing agent is polyester resin or liquid polyurethane curing agent.
According to the invention, the cross-linking agent is urea; the solvent is butanone. The leveling agent is an organic silicon surface additive; preferably, the leveling agent is a BYK-333 leveling agent. The wetting agent is at least one of BYK-181, BYK-187 and BYK-191. Preferably, the wetting agent is a mixture of BYK-181 and BYK-187 in a weight ratio of 2: 1. Preferably, the defoamer is an organosilicon defoamer, digao 1488, preferably the defoamer is tributyl phosphate or 2-ethylhexanol. The antioxidant is antioxidant 1010. Preferably, the diluent is one or more of ethyl acetate, butyl acetate, xylene, trimethylbenzene, tetramethylbenzene, isophorone, propylene glycol methyl ether acetate, and cyclohexanone.
Preferably, the nanoscale filler is one or more of nano silica, nano barium sulfate and nano calcium carbonate filler. Preferably, the dispersant is an SRE-4190 hyperdispersant. Preferably, an ultraviolet light absorber UV-9 is also included.
According to the invention, the temperature-sensitive color-changing powder is 6-color and 12-color temperature-sensitive color-changing powder; comprises various monochromatic temperature-sensitive color-changing powders of red, orange, yellow, green, blue and purple; it may be black, red, or blue thermochromic toner, for example. Preferably, the particle size of the temperature-sensitive color-changing powder is 4-8 μm. Preferably, the temperature sensing color changing temperature of the temperature sensing color changing powder is 30-50 ℃. Preferably, the temperature-sensitive color-changing powder mixed glue is epoxy resin AB glue or silica gel; the weight ratio of the epoxy resin AB glue to the temperature-sensitive color-changing powder is 1: 1.
According to the invention, the thermochromic ink also comprises long-acting noctilucent powder or noctilucent oil with the weight part of half of the thermochromic powder; the long-acting luminous powder or luminous oil is mixed with epoxy resin AB glue or silica gel, wherein the weight ratio of the epoxy resin AB glue or the silica gel to the long-acting luminous powder or luminous oil is 2: 1. Preferably, the long-acting luminous powder or luminous oil is mixed with baking varnish; the weight ratio of the baking varnish to the long-acting noctilucent powder or noctilucent oil is 2: 1.
According to the invention, the thermochromic ink also comprises long-acting incense powder or essence with one tenth of the thermochromic powder in parts by weight; the incense powder or essence is matched with epoxy resin AB glue or silica gel for use; the incense powder or essence is jasmine incense, sweet osmanthus incense, lemon incense, lavender incense, rose incense or wormwood incense or mint incense with mosquito repellent effect.
According to the present invention, a method for preparing a thermochromic ink includes the steps of: s1, stirring the connecting material, the cross-linking agent, the solvent, the flatting agent, the wetting agent and the diluent at the temperature of 60-75 ℃ for 25-35 minutes at 50-65 r/min, then magnetically stirring for 20-30 minutes at 100-150 r/min, and then standing for 25-45 minutes at room temperature to form a mixture; s2, adding temperature-sensitive color-changing powder, temperature-sensitive color-changing powder mixed glue, a defoaming agent, a dispersing agent, long-acting luminous powder or luminous oil and long-acting incense powder or essence into the mixture, dispersing and stirring at the temperature of 35-55 ℃ for 15-30 minutes at a speed of 100-150 r/min, adding a nanoscale filler and an antioxidant, and magnetically stirring at 200r/min for 15-30 minutes to stir uniformly; preferably, the method further comprises the step of adding the curing agent after stirring.
According to the invention, the method also comprises the step of adding the long-acting noctilucent powder or noctilucent oil, and long-acting incense powder or essence while stirring after adding the thermochromic powder.
According to the present invention, there is further included a step of pretreating the temperature-sensitive toner before use: dissolving gamma-methacryloxypropyltrimethoxysilane in acetone, spraying the acetone on the temperature-sensitive color-changing powder, uniformly mixing, and drying at 42-45 ℃ to obtain the modified temperature-sensitive color-changing powder.
The invention has the beneficial effects that:
by adopting the formula and the preparation method, the thermochromic ink with higher accuracy and sensitivity can be obtained, the problems that the conventional thermochromic ink is insensitive in color change, cannot realize rapid color change, is single in color change, is long in color compounding time and the like are solved, and the anti-counterfeiting effect is influenced. The thermochromic ink disclosed by the invention is high in air drying speed and drying speed, high in adhesive force, excellent in high-temperature and low-temperature resistance, sensitive in color change, free from the problems of migration, falling or reverse sticking and the like when being used for sticking the character anti-counterfeiting mark on an outer packaging box, and good in water resistance.
Detailed Description
The present invention will be described in further detail with reference to examples. These examples should not be construed as limiting the scope of the invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
The invention provides thermochromic ink which comprises the following components in parts by weight: 12-18 parts of a connecting material, 2.5-4.5 parts of a cross-linking agent, 45-78 parts of a solvent, 2.5-4 parts of a flatting agent, 1.0-3.5 parts of a wetting agent, 1-10 parts of a temperature-sensitive color-changing powder mixed glue, 8.5-12 parts of an antifoaming agent, 0-8 parts of a curing agent, 15-25 parts of a diluent, 1-3 parts of an antioxidant, 1-2.5 parts of a nano-grade filler, 1-3 parts of a dispersing agent and 1-10 parts of a temperature-sensitive color-changing powder.
Preferably, the thermochromic ink comprises the following components in parts by weight: 14-16 parts of a connecting material, 3-4 parts of a cross-linking agent, 50-70 parts of a solvent, 2.8-3.5 parts of a flatting agent, 1.5-3 parts of a wetting agent, 1.5-2 parts of an antioxidant, 10-11 parts of a defoaming agent, 2-3 parts of a curing agent, 18-22 parts of a diluent, 4-8 parts of a temperature-sensitive color-changing powder, 1.5-2.0 parts of a nano-grade filler, 1.5-2 parts of a dispersing agent and 4-8 parts of a temperature-sensitive color-changing powder mixed glue.
The thermochromic ink is also called liquid crystal color-changing ink, and is used for displaying different colors by temperature induction color change and different temperature induction. The source of the thermochromic powder is not limited, and the thermochromic powder can be sold in the market and can be microcapsule powder. The temperature-sensitive color-changing powder is 6-color or 12-color temperature-sensitive color-changing powder, comprises various monochrome temperature-sensitive color-changing powder of red, orange, yellow, green, blue and purple, and can also be black temperature-sensitive color-changing powder, red temperature-sensitive color-changing powder, blue temperature-sensitive color-changing powder and the like. Preferably, the temperature sensitive toner may have a particle size of 4 to 8 μm. The temperature sensing color change temperature of the temperature sensing color change powder is preferably 30-50 ℃. The liquid crystal is made of a substance similar to cholesterol, the molecular arrangement is deflected along with the temperature change, so that reversible bright and beautiful color change is presented, different colors can be displayed at different temperatures, and the color change can be red, orange, yellow, green, cyan, blue, purple and red for 12 times of color change processes. The thermochromic ink can be mixed with water in a mass ratio of 1:1 no matter whether the thermochromic ink is 12-color ink or 6-color ink, and different color changes can occur when the thermochromic ink is uniformly coated in a product to be designed.
Preferably, the temperature-sensitive color-changing powder mixed glue can be epoxy resin AB glue or silica gel, and the weight ratio of the epoxy resin AB glue to the temperature-sensitive color-changing powder is 1: 1. The temperature-sensitive color-changing powder can be mixed with the temperature-sensitive color-changing powder mixed glue and then added into the mixture.
According to the invention, the color-changing oilThe ink also comprises long-acting noctilucent powder or noctilucent oil which is half of the thermochromic powder in parts by weight. Wherein, the long-acting luminous powder or luminous oil can also be mixed with epoxy resin AB glue or silica gel according to the mass ratio of 2:1 for use. Preferably, the long-acting luminous powder or luminous oil can also be mixed with baking paint, and the weight ratio of the baking paint to the long-acting luminous powder or luminous oil is 2: 1. The luminous material comprises luminous powder with primary color, green light and blue light, luminous powder with various adjustable colors and luminous ink. The luminous powder may be also long-acting luminous powder of rare earth, belonging to long-lasting phosphor of alkaline earth aluminate type, and the composition is as follows: al (Al)2O3(Sr, Mg, Ca) O: (Eu, La and Dy) B can absorb light for 5-20 minutes under the irradiation of sunlight or lamplight, and then absorbed light energy is converted and stored in crystal lattices, and the energy can be converted into light energy to emit light, so that the light can be emitted effectively and continuously (the light emitting brightness is more than 10 mcd/m)2) The brightness of the light reaches 8-10 hours, and the light-emitting brightness is attenuated to the lower limit of human visual observation (0.32 mcd/m)2) The time can reach more than 70 hours, the chemical property is stable, the processes of light absorption, light storage and light emission can be repeatedly carried out, and the service life can reach more than 20 years.
UV color-changing material: ultraviolet light-changing powder, ink and photochromic material of various colors.
According to the invention, the thermochromic ink can also comprise long-acting incense powder or essence with one tenth of thermochromic powder in parts by weight; the incense powder or essence is matched with epoxy resin AB glue or silica gel for use; the incense powder or essence is jasmine incense, sweet osmanthus incense, lemon incense, lavender incense, rose incense or wormwood incense or mint incense with mosquito repellent effect.
The thermochromic effect is further divided into 12-color thermochromic effects (the colors can show red, orange, yellow, grass, green, purple, blue, clear, powder, blue, dark blue and green along with the change of temperature), 6-color thermochromic effects, namely, color-to-color thermochromic effects, color-to-colorless thermochromic effects, primary color noctilucent effects and mixed color noctilucent effects. The invention also has the color changing effect of ultraviolet UV and the color changing effect when meeting sunlight, and can also integrate the fragrance effect and the mosquito repelling effect by adding incense powder or essence and various materials with the mosquito repelling effect. The thermochromic ink can also have the effect of imitating beeswax, can be mixed with epoxy resin AB glue and pearly oil color paste or oil color concentrate and uniformly blended, and can be internally provided with micro-embedded accessories, such as metal computer sheets, copper, stainless steel sheets (obtained by cutting a stainless steel sheet cutting machine), dry flowers (plant flowers are dried) glitter powder or paillettes and the like.
According to the invention, the binder is a transparent thermosetting resin, and can be one or more of epoxy resin, acrylic resin and polyurethane resin. Preferably, the viscosity of the binder is 8-10Pa.S/30 ℃.
Preferably, in order to enhance the adhesion of the ink to the substrate, the ink system may further comprise a curing agent, and the curing agent may be one or more of imidazoles, acid anhydrides, polyester resins, liquid polyurethanes and polyisocyanates. The curing agent and the binder are matched to form a two-component system, and when the binder is epoxy resin, the curing agent is imidazole, acid anhydride, polyester resin or liquid polyurethane curing agent; when the connecting material is polyurethane resin and/or hydroxyl acrylic resin, the curing agent component is polyisocyanate; when the main body of the binder is epoxy acrylic resin, the curing agent is polyester resin or liquid polyurethane curing agent.
According to the invention, the cross-linking agent can be urea, and the urea is used as the cross-linking agent, so that the adhesive property and the water resistance of the binder can be improved. The solvent may be butanone. The leveling agent is an organic silicon surface additive. Preferably, the leveling agent is a BYK-333 leveling agent. The wetting agent can be at least one of BYK-181, BYK-187, and BYK-191. In a preferred embodiment of the present invention, the wetting agent is a mixture of BYK-181 and BYK-187 in a weight ratio of 2: 1. Further, in a preferred embodiment of the present invention, the leveling agent is an organosilicon surface additive, and further, the leveling agent is a BYK-333 leveling agent.
Preferably, the defoamer is an organosilicon defoamer, digao 1488, preferably the defoamer is tributyl phosphate or 2-ethylhexanol. The antioxidant is antioxidant 1010. Preferably, the diluent is one or more of ethyl acetate, butyl acetate, xylene, trimethylbenzene, tetramethylbenzene, isophorone, propylene glycol methyl ether acetate, and cyclohexanone. The dispersant may be an SRE-4190 hyperdispersant.
According to the invention, the defoaming agent and the dispersing agent are added into the thermochromic ink, so that the thermochromic powder is uniformly dispersed in the ink, and the influence on the thermochromic performance of the thermochromic ink caused by foam generated in the preparation and use processes of the ink is prevented. The dispersing agent can effectively improve the precipitation problem of the thermochromic powder after standing, so that the dispersibility of the thermochromic powder in the ink is kept stable.
Preferably, the nanoscale filler is one or more of a nano silica, a nano barium sulfate and a nano calcium carbonate filler. The filler is in a nanometer level, so that the rheological property and the vividness of the ink are facilitated, and the filler is beneficial to being cooperated with the binder to endow the ink with excellent characteristics in the aspects of printability, color and luster of printed products, physical resistance and ink stability.
Preferably, an ultraviolet light absorber UV-9 may also be included, in conventional amounts.
According to another aspect of the present invention, there is also provided a method for preparing a thermochromic ink, comprising the steps of: s1, stirring the connecting material, the cross-linking agent, the solvent, the flatting agent, the wetting agent and the diluent at the temperature of 60-75 ℃ for 40-55 minutes, and then standing for 25-45 minutes to form a mixture; s2, adding a defoaming agent and a dispersing agent into the mixture, stirring and mixing for 15-30 minutes, adding temperature-sensitive color-changing powder and temperature-sensitive color-changing powder mixed glue, stirring for 10-20 minutes, then adding a nano-grade filler and an antioxidant, and uniformly stirring; preferably, a step of adding the curing agent after adding the temperature sensitive reversible toner is further included.
Preferably, the method also comprises the step of adding the long-acting noctilucent powder or noctilucent oil, and long-acting incense powder or essence after adding the thermochromic powder and stirring.
According to the present invention, there is further included a step of pretreating the temperature-sensitive toner before use: dissolving gamma-methacryloxypropyltrimethoxysilane in acetone, spraying the acetone on the temperature-sensitive color-changing powder, uniformly mixing, and drying at 42-45 ℃ to obtain the modified temperature-sensitive color-changing powder.
The invention can also realize the interconversion of the color water of the printing pattern from one color to another color, rather than the reciprocal of only from color to colorless, by adding the temperature-sensitive color-changing powder and the color-invariant component into the ink and generating the color-changing effect through the mutual interaction and mutual superposition of the two components. Meanwhile, the temperature-sensitive color-changing powder is subjected to surface modification, so that the temperature-sensitive color-changing powder has better compatibility in a coating, and the adhesive force, weather resistance and other properties of the ink are excellent. The temperature-sensitive color-changing powder is subjected to surface modification to improve the compatibility of the temperature-sensitive color-changing powder in a matrix coating, and printed pictures and texts can change color (or fade) or recover primary color after reaching a certain temperature point through temperature sensing, friction or contact, so that the effect is more obvious and rapid compared with other common temperature-sensitive color-changing powder.
The technical scheme of the invention is further explained by combining specific examples.
Example 1
Formula (by weight): the adhesive is 14 parts of polyurethane resin (viscosity is 10Pa.S/30 ℃), 3 parts of cross-linking agent urea, 50 parts of butanone serving as a solvent, 2.8 parts of BYK-333 leveling agent, 3 parts of mixed wetting agent consisting of BYK-181 and BYK-187 in a weight ratio of 2:1, 2 parts of antioxidant 1010, 10 parts of defoaming agent tributyl phosphate, 2 parts of curing agent polyisocyanate, 18 parts of diluent butyl acetate, 8 parts of temperature-sensitive variable color powder, 8 parts of epoxy resin AB glue, 2.0 parts of nano silicon dioxide and 2 parts of SRE-4190 hyper-dispersant.
The preparation method comprises the following steps:
(1) pretreating the temperature-sensitive color-changing powder: dissolving gamma-methacryloxypropyltrimethoxysilane in acetone, spraying the acetone on the temperature-sensitive color-changing powder, uniformly mixing, and drying at the temperature of 45 ℃ to obtain the modified temperature-sensitive color-changing powder. And magnetically stirring and uniformly mixing the modified temperature-sensitive color-changing powder and the temperature-sensitive color-changing powder mixed glue at the rotating speed of 30r/min for 20 minutes to obtain a mixed material.
(2) Mixing the connecting material, the cross-linking agent, the solvent, the leveling agent, the wetting agent and the diluent at 75 ℃, firstly magnetically stirring for 25 minutes at 60r/min, then magnetically stirring for 30 minutes at 150r/min, and then standing for 45 minutes at room temperature to form a mixture;
(3) adding the mixture obtained in the step (1) into the step (2), adding a defoaming agent, a dispersing agent, long-acting noctilucent powder or noctilucent oil and long-acting incense powder or essence, dispersing and stirring at 130r/min, stirring for 15 minutes at 40 ℃, then adding a nanoscale filler and an antioxidant, magnetically stirring for 20 minutes at 200r/min, adding a curing agent, and uniformly mixing.
Example 2
Formula (by weight): the adhesive is 16 parts of epoxy acrylic resin (the viscosity is 8Pa.S/30 ℃), 4 parts of cross-linking agent urea, 70 parts of butanone serving as a solvent, 3.5 parts of BYK-333 leveling agent, 1.5 parts of wetting agent BYK-191, 1.5 parts of antioxidant 1010, 11 parts of defoaming agent 2-ethylhexanol, 3 parts of curing agent polyester resin, 22 parts of diluent propylene glycol monomethyl ether acetate, 7 parts of thermochromic powder, 8 parts of epoxy resin AB adhesive, 1.5 parts of nano calcium carbonate and 1.5 parts of SRE-4190 hyperdispersant.
The preparation method comprises the following steps:
(1) pretreating the temperature-sensitive color-changing powder: dissolving gamma-methacryloxypropyltrimethoxysilane in acetone, spraying the acetone on the temperature-sensitive color-changing powder, uniformly mixing, and drying at 42 ℃ to obtain the modified temperature-sensitive color-changing powder. And magnetically stirring and uniformly mixing the modified temperature-sensitive color-changing powder and the temperature-sensitive color-changing powder mixed glue at the rotating speed of 30r/min for 20 minutes to obtain a mixed material.
(2) Mixing the connecting material, the cross-linking agent, the solvent, the flatting agent, the wetting agent and the diluent at 60 ℃, firstly magnetically stirring for 30 minutes at 50r/min, then magnetically stirring for 30 minutes at 130r/min, and then standing for 40 minutes at room temperature to form a mixture;
(3) adding the mixture obtained in the step (1) into the step (2), adding a defoaming agent, a dispersing agent, long-acting noctilucent powder or noctilucent oil, long-acting incense powder or essence and an ultraviolet color-changing powder, mixing epoxy resin AB glue and pearly oil color paste or oily color concentrate (conventional amount) uniformly, dispersing and stirring at 55 ℃ for 30 minutes at 130r/min, then adding a nanoscale filler and an antioxidant, magnetically stirring at 200r/min for 30 minutes, adding a curing agent, and uniformly mixing.
Example 3
The formula and the preparation method are the same as those of the example 2, except that the thermochromic powder is not pretreated in the step (1).
Example 4
The formulation and preparation method are the same as example 2, except that the weight parts of the components in the formulation are not within the scope of the invention, and the formulation is as follows:
the adhesive is 10 parts of epoxy acrylic resin (the viscosity is 6Pa.S/30 ℃), 6 parts of cross-linking agent urea, 30 parts of butanone, 6 parts of BYK-333 leveling agent, 0.5 part of wetting agent BYK-191, 0.5 part of antioxidant 1010, 6 parts of defoaming agent 2-ethylhexanol, 10 parts of curing agent polyester resin, 10 parts of diluent propylene glycol monomethyl ether acetate, 20 parts of thermochromic powder, 15 parts of epoxy resin AB glue, 5 parts of nano calcium carbonate and 5 parts of SRE-4190 hyper-dispersant.
Comparative example 1
The formula is as follows: 19 parts of polyvinyl alcohol, 2 parts of modified rosin resin, 2.44 parts of urea, 63.41 parts of deionized water, 9.76 parts of tributyl phosphate, 0.73 part of wetting agent (PE-100), 1.66 parts of BYK-333 leveling agent, 2.5 parts of temperature-sensitive reversible toner and 2.5 parts of auxiliary agent (silica sol and chitosan quaternary ammonium salt in a mass ratio of 4: 1).
The preparation method comprises the following steps: (1) and (3) placing the temperature-sensitive reversible color-changing powder in 0.7g/L dopamine solution, adjusting the pH value to 8, adding 0.14g lignosulfonate, stirring for reacting for 4h, separating and drying.
(2) Stirring the connecting material, the cross-linking agent, the solvent, the leveling agent and the wetting agent at a constant temperature of 90 ℃ for 25 minutes at a speed of 160r/min, and standing for 20 minutes to form a mixture of a milky white sol system;
(3) and (3) adding a defoaming agent into the mixture obtained in the step (2), stirring and mixing at a constant temperature of 55 ℃ for 10 minutes at a speed of 50 r/minute, cooling to 35 ℃, adding a temperature-sensitive color-changing powder (38 ℃) and an auxiliary agent, stirring for 5 minutes, and completely dispersing the materials to obtain the ink.
Comparative example 2
The formula is as follows: 15 parts of polyvinyl alcohol, 1.5 parts of modified rosin resin, 3 parts of urea, 65 parts of deionized water, 11 parts of tributyl phosphate, 1.05 parts of wetting agent (PE-100), 1.86 parts of BYK-333 leveling agent, 2.5 parts of temperature-sensitive reversible toner and 2.5 parts of auxiliary agent (silica sol and chitosan quaternary ammonium salt in a mass ratio of 4: 1).
The preparation method comprises the following steps: (1) and (3) placing the temperature-sensitive reversible color-changing powder in 0.7g/L dopamine solution, adjusting the pH value to 8, adding 0.14g lignosulfonate, stirring for reacting for 4h, separating and drying.
(2) Stirring the connecting material, the cross-linking agent, the solvent, the leveling agent and the wetting agent at a constant temperature of 90 ℃ for 25min at a speed of 160r/min, and standing for 20min to form a mixture of a milky white sol system;
(3) and (3) adding a defoaming agent into the mixture obtained in the step (2), stirring and mixing at a constant temperature of 55 ℃ for 10min at a speed of 50r/min, cooling to 35 ℃, adding a temperature-sensitive reversible toner (38 ℃) and an auxiliary agent, stirring for 5min, and obtaining the ink after the materials are completely dispersed.
The inks prepared in examples 1 to 4 and comparative examples 1 to 2 were applied to a board to be tested (e.g., a wood board, a toy) and air-dried for 3min using a hot air fan having an air speed of 6m/s and a temperature of 60 ℃. And then carrying out performance detection:
(1) the air drying speed test method comprises the following steps:
a. has no stickiness. The ink was not sticky to the touch.
b. No stickiness when twisted by thumb. The ink film was not broken by rotational twisting with the thumb on the ink film with about 2kg of downward pressure. (expressed as rank good x)
c. And (4) no scratch and curing. The ink film is scratched by a fingernail without cracking.
d. And (4) no scratch and curing. The ink film is scratched by a fingernail without cracking.
According to the number of grades from difference to optimum, the more the grades are, the higher the grade is, the better the performance is.
(2) The adhesive force test method comprises the following steps: the ink film is wiped back and forth by an eraser for 10-15 times, and the ink film is divided into several grades according to whether the ink film can be wiped off or not, if the ink film can be wiped off basically, a small amount of the ink film is wiped off, a few ink films are wiped off and hardly fall off, and the number of the ink films is used for indicating the quality, and the number of the ink films is used for indicating the excellent performance.
(3) And (3) a high-temperature resistance test method:
and (3) folding the tested printing part in a cross shape, folding the edge, pressurizing a weight of 2kg, placing the weight into a constant temperature box at 60 ℃ for testing for 8 hours, taking out the sample, opening and checking. The ink film is wiped back and forth by an eraser for 10-15 times, and the ink film can be wiped off basically, a small amount of the ink film is wiped off, the ink film hardly drops off, the ink film is divided into several grades, the quality is represented by the number of the ink film, and the performance is represented by the number of the ink film.
(4) The low temperature resistance detection method comprises the following steps:
and (3) after the tested printing part is positioned in a cross-shaped folded state, pressing a 2kg weight at the folded edge, placing the folded product into a refrigerator at the temperature of-10 ℃ for testing for 8 hours, taking out the sample, and opening and checking. The ink film is wiped back and forth by an eraser for 10 to 15 times, the ink film can be basically wiped off, a small amount of ink film is wiped off, a very small amount of ink film is wiped off, no ink film falls off, the ink film is graded into a plurality of grades, the quality is represented by the number of the ink film, and the performance is represented by the number of the ink film.
(5) The detection method of temperature-sensitive discoloration comprises the following steps:
the printed part to be detected is closely attached to a thermal resistor, a thermal resistor temperature sensing head is connected with a digital display temperature control instrument, and for example, red temperature sensing powder capable of yellowing at 38 ℃ is selected. The digital temperature control instrument was turned on, the room temperature was displayed (assuming room temperature 25 ℃ C.), and the temperature was set at 38 ℃. When the thermal resistor is heated to 38 ℃ (if the room temperature is lower, the temperature can be properly increased by 0.1-0.5 ℃ because the thermal resistor dissipates heat to the environment faster), the yellow color of the printing part is not changed, the yellow color of the printing part is changed into the red color and is not very clear, the yellow color of the printing part is changed into the red color and is obviously visible, the yellow color of the printing part is changed into the deep red color, and the change is obviously represented by a plurality of numbers.
(6) And (3) package simulation test:
and sticking the printed character anti-counterfeiting mark on an outer packaging box, standing at normal temperature for 3-6 months after sticking, and determining whether the water-based ink has the bad phenomena of migration, falling off or reverse sticking and the like. The ink is graded according to the severity of ink migration, falling off or reverse pasting, wherein the number of the ink is used for representing that the ink is easy to migrate and fall off or reverse pasting, and the number of the ink is used for representing that the ink is not easy to fall off or reverse pasting, so that the performance is good.
(7) And (3) testing the water resistance:
after the printed paper is placed for one day, the printed paper is wiped back and forth for 10-15 times by force of a cotton swab dipped with water on the ink film, and according to the fact that a large amount of pigment is stuck on the cotton swab, a small amount of pigment is stuck on the cotton swab, and no pigment is stuck on the cotton swab, the number of the pigment is represented by the number, the number of the pigment on the cotton swab is small, the number of the pigment on the cotton swab is large, the number of the pigment on the cotton swab is small, and the performance is good.
The test results are shown in table 1.
TABLE 1 test results
As can be seen from Table 1, the thermochromic ink prepared by adopting the formula, the parts by weight and the preparation method of the invention has more excellent performance compared with the existing ink.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. The thermochromic ink is characterized by comprising the following components in parts by weight:
12 to 18 parts by weight of binder, 2.5 to 4.5 parts by weight of cross-linking agent
45-78 parts by weight of solvent and 2.5-4 parts by weight of leveling agent
1.0-3.5 parts by weight of wetting agent and 1-3 parts by weight of antioxidant
8.5-12 parts of defoaming agent and 0-8 parts of curing agent
15-25 parts of diluent and 1-10 parts of thermochromic powder
1-2.5 parts of nanoscale filler and 1-3 parts of dispersant
1-10 parts by weight of thermochromic powder mixed glue.
2. The thermochromic ink according to claim 1, comprising the following components in parts by weight:
14-16 parts of binder and 3-4 parts of cross-linking agent
50-70 parts by weight of solvent and 2.8-3.5 parts by weight of leveling agent
1.5-3 parts of wetting agent and 1.5-2 parts of antioxidant
10-11 parts of defoaming agent and 2-3 parts of curing agent
18-22 parts of diluent and 4-8 parts of thermochromic powder
1.5-2.0 parts by weight of nano-grade filler and 1.5-2 parts by weight of dispersing agent
4-8 parts of thermochromic powder mixed glue.
3. The thermochromic ink according to claim 1 or 2, wherein the binder is a transparent thermosetting resin comprising one or more of an epoxy resin, an acrylic resin and a urethane resin; preferably, the viscosity of the connecting material is 8-10Pa.S/30 ℃;
preferably, the curing agent is one or more of imidazoles, acid anhydrides, polyester resin, liquid polyurethane and polyisocyanate; the curing agent and the binder are matched to form a two-component system, and when the binder is epoxy resin, the curing agent is imidazole, acid anhydride, polyester resin or liquid polyurethane curing agent; when the connecting material is polyurethane resin and/or hydroxyl acrylic resin, the curing agent component is polyisocyanate; when the main body of the binder is epoxy acrylic resin, the curing agent is polyester resin or liquid polyurethane curing agent.
4. The thermochromic ink according to any of claims 1 to 3, wherein the cross-linking agent is urea; the solvent is butanone;
the leveling agent is an organic silicon surface additive; preferably, the leveling agent is a BYK-333 leveling agent;
the wetting agent is at least one of BYK-181, BYK-187 and BYK-191;
preferably, the wetting agent is a mixture of BYK-181 and BYK-187 in a weight ratio of 2: 1;
preferably, the defoamer is an organosilicon defoamer, diho 1488, preferably the defoamer is tributyl phosphate or 2-ethylhexanol;
the antioxidant is 1010;
preferably, the diluent is one or more of ethyl acetate, butyl acetate, xylene, trimethylbenzene, tetramethylbenzene, isophorone, propylene glycol methyl ether acetate and cyclohexanone;
preferably, the nanoscale filler is one or more of nano silica, nano barium sulfate and nano calcium carbonate filler; preferably, the dispersant is an SRE-4190 hyperdispersant;
preferably, an ultraviolet light absorber is also included, which is UV-9.
5. The thermochromic ink according to any one of claims 1 to 4,
the temperature-sensitive color-changing powder is 6-color and 12-color temperature-sensitive color-changing powder; comprises various monochromatic temperature-sensitive color-changing powders of red, orange, yellow, green, blue and purple; or black temperature-sensitive color-changing powder, red temperature-sensitive color-changing powder or blue temperature-sensitive color-changing powder and the like; preferably, the particle size of the temperature-sensitive color-changing powder is 4-8 μm; preferably, the temperature sensing color changing temperature of the temperature sensing color changing powder is 30-50 ℃;
preferably, the temperature-sensitive color-changing powder mixed glue is epoxy resin AB glue or silica gel; the weight ratio of the epoxy resin AB glue to the temperature-sensitive color-changing powder is 1: 1.
6. The thermochromic ink according to any one of claims 1 to 4, further comprising long-acting luminescent powder or luminescent oil in a weight part which is half of the thermochromic powder; the long-acting luminous powder or luminous oil is mixed with epoxy resin AB glue or silica gel, wherein the weight ratio of the epoxy resin AB glue or the silica gel to the long-acting luminous powder or luminous oil is 2: 1;
preferably, the long-acting luminous powder or luminous oil is mixed with baking varnish; the weight ratio of the baking varnish to the long-acting noctilucent powder or noctilucent oil is 2: 1.
7. The thermochromic ink according to any one of claims 1 to 6, further comprising a long-acting fragrance or essence in parts by weight that is one tenth of the thermochromic powder; the incense powder or essence is matched with epoxy resin AB glue or silica gel for use; the incense powder or essence is jasmine incense, sweet osmanthus incense, lemon incense, lavender incense, rose incense or wormwood incense or mint incense with mosquito repellent effect.
8. The method for producing a thermochromic ink according to any of claims 1 to 7, characterized by comprising the steps of:
s1, stirring the connecting material, the cross-linking agent, the solvent, the flatting agent, the wetting agent and the diluent at the temperature of 60-75 ℃ for 25-35 minutes at 50-65 r/min, then magnetically stirring for 20-30 minutes at 100-150 r/min, and then standing for 25-45 minutes at room temperature to form a mixture;
s2, adding temperature-sensitive color-changing powder, temperature-sensitive color-changing powder mixed glue, a defoaming agent, a dispersing agent, long-acting luminous powder or luminous oil and long-acting incense powder or essence into the mixture, dispersing and stirring at the temperature of 35-55 ℃ for 15-30 minutes at a speed of 100-150 r/min, adding a nanoscale filler and an antioxidant, and magnetically stirring at 200r/min for 15-30 minutes to stir uniformly; preferably, the method further comprises the step of adding the curing agent after stirring.
9. The method for preparing a thermochromic ink according to claim 8, further comprising the step of adding the thermochromic powder and then adding the long-acting luminescent powder or luminescent oil, long-acting fragrance powder or essence while stirring.
10. The production method according to claim 8 or 9, characterized by further comprising a step of pretreating the temperature-sensitive color-changing powder before use: dissolving gamma-methacryloxypropyltrimethoxysilane in acetone, spraying the acetone on the temperature-sensitive color-changing powder, uniformly mixing, and drying at 42-45 ℃ to obtain the modified temperature-sensitive color-changing powder.
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| CN115157736A (en) * | 2022-07-04 | 2022-10-11 | 厦门雅瑞实业有限公司 | A kind of color-changing glasses and preparation method thereof |
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| CN115287011A (en) * | 2022-08-25 | 2022-11-04 | 国网湖北省电力有限公司咸宁供电公司 | Temperature-sensing color-changing insulating packaging material for electrical insulation |
| CN116042019A (en) * | 2023-02-23 | 2023-05-02 | 重庆宏图新材料科技有限公司 | Environment-friendly ink special for temperature change of food packaging bag and preparation method thereof |
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| CN117301744A (en) * | 2023-10-07 | 2023-12-29 | 湖北广彩印刷有限公司 | Low-emission environment-friendly printing process |
| CN117301744B (en) * | 2023-10-07 | 2024-04-02 | 湖北广彩印刷有限公司 | Low-emission environment-friendly printing process |
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